The copolymerization of 3-thienylmethyl disulfide and benzyl disulfide has been investigated. Two monomers were synthesized in a novel facile way. Copolymer of them, especially poly (3-thienylmethyl disulfide-co-benzyl disulfide), ratio 1 : 4, namely, TcB1:4, was easily electrocopolymerized to form a stable and higher conductive structure at a lower potential on Pt, Au, or glass carbon electrode. TcB1:4 and TcB4:1, especially the former, exhibit better conductivities than those of pure poly 3-thienylmethyl disulfide and poly benzyl disulfide. The copolymer has larger areas than that of monopolymer by cyclic voltammogram measurement. The copolymer shows a capability Of Supplying more power and energy than monopolymer itself. Copolymers could be used as cathode materials for lithium secondary batteries because their functional groups could not be destroyed before 80 degrees C. In scanning electron micrography, the copolymers show larger compacter structure. The results of the copolymer systems show that they are potentials as cathode materials for lithium batteries. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 116: 727-735, 2010